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Research Progress on Yb3+-doped Scintillation Crystals
PAN Shang-Ke,YANG Pei-Zhi
2005 Vol. 20 (5): 10251031
Abstract(
1908 )
PDF(473KB)(
1544
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The Yb3+-doped scintillation crystals are novel kinds of scintillators, which may be applied to the detection of the solar neutrinos. This paper briefly introduced the mechanism of charge transfer luminescence in scintillators containing Yb3+ ions, and the host effect on the thermal and concentrations quenching. This paper also reviewed the research development of Yb3+-doped garnet and perovskite crystals, especially on the growth, scintillation properties and promising application of Yb:YAG and Yb:YAP crystals. Finally the future research topics of the Yb3+-doped scintillation crystals were discussed.
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Luminescent Characteristics of ZrO2 and ZrO2:Dy3+ Nanocrystals
YUE Ming-Xin,LI Dian-Chao,YU Li-Xin,WANG Yan
2005 Vol. 20 (5): 10321036
Abstract(
1799 )
PDF(330KB)(
1088
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ZrO2:Dy nanocrystals with different sizes and concentrations of Dy3+ were prepared with the precipation method. The results indicate that the broad excitation and emission bands in ZrO2 nanocrystals occur, which are associated with the electron transition between valence and conduction bands. In Dy3+ doped samples, the luminescent intensity increases with the increase of particle sizes. The emission intensity of Dy3+ for co-doped Dy3+/Li+ ZrO2 dramatically increases. As the concentration of Dy3+ varies, the intensity ratio of yellow to blue emission changes, and the concentration quenching is originated from the exchange interaction.
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Synthesis and Sinterability of YAG Nanopowders by Microwave Homogeneous Precipitation
WANG Jie-Qiang,TAO Wen-Hong,GAO Xin-Rui,LI Yong2,ZHENG Shao-Hua
2005 Vol. 20 (5): 10371042
Abstract(
2120 )
PDF(386KB)(
1400
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The low-agglomerated single-phase YAG nanopowders were synthesized by the microwave homogeneous precipitation in the presence of urea. The composition and transformations during calcination of YAG precursor were analyzed by IR, DTA/TG and XRD. The size and morphology of YAG powders were characterized by LD and TEM. Results show that the amorphous precursor crystallizes directly to single-phase YAG powders upon calcining to 900℃ that was synthesized under [urea]/[metal ions] molar ratio of 15. The size distribution and sinterability of YAG powders are obviously improved by adding (NH4)2SO4 into the reaction solution. YAG powders obtained from the precursor with the (NH4)2SO4 content of 8% have good sinterability and can be highly densified at 1500℃.
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Synthesis and Its Hydrolyzation, Thermal Stability and Rare Earth Activated Luminescent Properties of Ba3BPO7
DUAN Cheng-Jun,WU Xue-Yan,CHEN Hao-Hong,YANG Xin-Xin,ZHAO Jing-Tai
2005 Vol. 20 (5): 10431048
Abstract(
1884 )
PDF(354KB)(
1261
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We explored the synthesis methods of Ba3BPO7 by the high temperature solid reaction method; single phase of Ba3BPO7 was obtained with 3:1 molar ratio of BaCO3 and BPO4, 3:1:1molar ratio of BaCO3, NH4H2PO4 and H3BO3, 2:1:1 molar ratio of BaCO3, BaHPO4 and H3BO3, respectively. The hydrolyzation and thermal stability properties of Ba3BPO7 were investigated. The results show that Ba3BPO7 can react with water and form the final products of Ba3(PO4)2, Ba5(PO4)3OH and Ba(OH)2; TG-DTA shows that it melts congruently and its melting point is about 1353℃. The X-ray excited luminescent properties of Ba3BPO7 with rare earth activated were also investigated. The results show that there is energy transfer between the host and rare earth ions.
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Effect of Sr2+ Substitution for Equivalent Ca2+ Ions on Luminescence Intensity of CaTiO3:0.002Pr3+
PENG Li-Xia,HONG Zhang-Lian,ZHOU Shi-Feng,WANG Min-Quan
2005 Vol. 20 (5): 10491053
Abstract(
2170 )
PDF(213KB)(
1199
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Red phosphors (Ca1-xSrx)TiO3:0.002Pr3+ (x=0~0.6) were prepared by solid state reaction route and their properties were investigated by photoluminescence (PL) spectra and XRD, respectively. All samples have a red emission peak at 612nm due to the intra-4f transition of Pr3+ from 1D2 to 3H4 state. The results indicate that both emission intensity and a axis parameter show an extremum at x=0.15: the emission intensity is enhanced about 3 times, and the lattice parameter of a axis shows a minimum value. The results show that, besides the charge defects induced by unequilvalent ion substitution, the equilvalent Sr2+ substitution for Ca2+ can also influence the emission intensity through the crystal structure evolution.
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Preparation of Core-shell Structural Zirconia Coated Alumina Nanocomposite Powders
YU Jian-Chang
2005 Vol. 20 (5): 10541058
Abstract(
2374 )
PDF(500KB)(
1644
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A zirconia coated alumina nanocomposite was synthesized by the one-step alkoxide hydrolyzing method. A layer of very uniform nanocrystalline zirconia shell with its thickness about 4~5nm was successfully coated onto the commercial nano-alumina particle. The thickness of the zirconia layer can be controllable by adjusting the concentrations of zirconium source and acetic acid. The results show that such novel core-shell nanocomposite powders of alumina-zirconia can be helpful to inhibit the much faster growth of alumina particles and show the uniform surface morphogenesis. XRD, TEM, FESEM and EDS were used for the structural characterizations.
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Synthesis and Mossbauer Characteristic of Cobalt Bearing Ferrite Particles
WANG-Jing,DENG-Tong,YANG-Huan,DAI Yu-Jie
2005 Vol. 20 (5): 10591065
Abstract(
1907 )
PDF(438KB)(
1224
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Cobalt bearing magnetite particles were synthesized by aerial oxidation of ferrous and cobalt ions at alkaline condition and room temperature. The samples obtained at different intervals during reaction were characterized by XRD and IR. The cobalt-bearing ferrites were produced through the green-rust intermediate phase. Different compounds were synthesized by using Co2+/Fe3+ starting ratios of 1/20, 1/15, 1/10, 1/7, 1/5 and 1/3, and Co-ferrites with Co/Fe ratios of 0.05,0.06,0.08, 0.12, 0.17, 0.18 were obtained. The chemical composition and microstructure of those precipitates were characterized by chemical analysis and XRD. Meanwhile, further information of the producing process was confirmed by Mossbauer analysis. The results reveal that in the conditions of room temperature Co2+ will replace Fe3+ at octahedral positions in the spinel structure, and the increase of Co in initial solution is disadvantageous to the formation of the spinel structure. The non-magnetic ferric oxide is included in the compound containing Co outside the green-rust system.
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Preparation and Characterization of Rod-like γ-Fe2O3 Nanoparticles
JIANG Guo-Hua,JIANG Ji-Sen
2005 Vol. 20 (5): 10661070
Abstract(
1982 )
PDF(375KB)(
1160
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This paper presented a new method to prepare γ-Fe2O3 nanoparticles. After the reaction of FeCl3 with NaOH in the presence of polyethylene glycol(PEG-400), the precipitate was dried at 60℃ in air and then calcined at different temperatures for 1h. XRD, Mossbauer spectroscope, TEM, FTIR and TG-DTA were used to characterize the obtained samples. The results show that after the precipitate dried at 60℃ for 6h, a poor-crystalline γ-Fe2O3 powder forms, and calcined at 300℃ for 1h, the poor-crystalline powder turns to rod-like γ-Fe2O3 nanoparticles with aspect ratio about 5.
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In Situ Combination and Phase Formation of Sol-Gel Derived PbTiO3/(Ni,Pb) Ferrite Multiphase Powders
DONG Yan-Ling,DU Pi-Yi,WENG Wen-Jian,HAN Gao-Rong
2005 Vol. 20 (5): 10711076
Abstract(
1845 )
PDF(613KB)(
1351
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Ferroelectric/ferromagnetic multiphase composite powders consisting of PbTiO3 as ferroelectricity and NiFe2O4 (PbFe12O19) as ferromagnetism were successfully formed in situ by the sol-gel method. The phase structure was measured by XRD and the morphology was observed by SEM. The results show that the biphase composite powder consisting of PbTiO3 and NiFe2O4 are formed at - 700℃ and the triphase composite powder consisting of PbTiO3, NiFe2O4 and PbFe12O19, above 750℃ in situ in alead-acetate/tetrabutyl-titanate/nickel-acetate/ferric-nitrate precursor system. The forming and growing processes are dependent on the calcination temperatrues of the powders. In addition, the phases coexisting in the composite system are mostly in forms of solid solutions, and the lattice constant of each phase varies with the different amount of phase solubility.
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Synthesis and Electromagnetic Properties of Ni0.8Zn0.2Fe2O4 Nanocrystalline
SUN Jie,LIU Jian-Hua,LI Song-Mei
2005 Vol. 20 (5): 10771082
Abstract(
2027 )
PDF(425KB)(
2440
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The nanocrystalline Ni0.8Zn0.2Fe2O4 was synthesized by a sol-gel auto-combustion method using citric acid as the chelating agents. The analysis methods of FT-IR, XRD, DSC-TG, TEM, wave-guide were used to character the gel and the products. The phenomena of melt, combustion and forming crystal for gel were investigated in the processes of thermo-decomposition. The results show that metal ions and carboxyl are coordinated by the oriented manner. The temperature of decomposition for the gel is 220℃, and the nanocrystalline is formed after the combustion of the gel. The mixture, which consists of Ni0.8Zn0.2Fe2O4 nanocrystalline and paraffin, has both dielectric loss and magnetic loss in the frequency range of 8~12GHz. The reflectivity of spinel nanocrystalline increases and the reflectivity absorption peaks shift from high frequency to low frequency with the increase of thickness.
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Removal of OH Groups in Er3+)-doped Phosphate Glasses by Reaction Atmosphere Process
YANG Gang-Feng,ZHAO San-Yin,DENG Zai-De,SUN Jia-Sen,JIANG Zhong-Hong
2005 Vol. 20 (5): 10831088
Abstract(
2264 )
PDF(499KB)(
1302
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Er3+-doped phosphate glasses with various concentrations of OH groups were fabricated. The effects of technological parameters on result of Reaction Atmosphere Process were investigated. The dehydrate process was discussed by thermodynamic theory of open system. The results show that the dehydration reagent in the bubbling gas is the main dynamic force of dehydration reaction, and the OH groups are removed rather rapidly at the initial stage. Elevating temperature and increasing bubbling flux can conduce to the increase of dehydration efficiency. The rate of dehydration in the glass melt is affected by ‘cage effect’. The dehydration rate is controlled by the probability of forming encounter twins between OH and CCl4.
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Characterization on the Optical Properties of Large PbWO4:(Sb,Y) Crystal
XIE Jian-Jun,YUAN Hui,YANG Pei-Zhi,SHEN Bing-Fu,CAO Dun-Hua,LIAO Jing-Ying,GU Mu,YIN Zhi-Wen
2005 Vol. 20 (5): 10891094
Abstract(
1535 )
PDF(285KB)(
1205
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This paper presents the characterization and investigation of the optical properties on doubly-doped large PbWO4:(Sb,Y) crystals grown by the modified Bridgman method. Based on the comparison
measurement of the optical transmission spectra, X-ray excited luminescence, photoluminescence, decay time, light yield and irradiation damage for 23mm×23mm×20mm crystal samples
cut from seed end, middle part and top end of a large PbWO4:(Sb,Y) crystal ingot, the results show that co-doping Sb and Y can significantly improve the light yield, radiation hardness and other spectroscopic properties of PbWO4 crystal. However, the uniformity of large PbWO4:(Sb,Y) crystal needs to be further improved based on the comparison of measurement results.
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Decolorisation and Decarbonisation Study on Sapphire Grown by TGT
XU Jun,ZHOU Guo-Qing,DENG Pei-Zhen,SI Ji-Liang,QIAN Xiao-Bo,ZHOU Yong-Zhong,WANG Yin-Zhen,ZHOU Sheng-Ming,ZHU Ren-Yuan
2005 Vol. 20 (5): 10951098
Abstract(
1681 )
PDF(331KB)(
1519
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The sapphire boule grown by TGT is a bit colorful due to the volatilization of graphite heater at high temperature and absorptions of transitional metal ions in raw material. It is light red at the shoulder and little yellow at the bottle of the sapphire boule, respectively. The as-grown sapphire boule (φ110×80mm3) turns out colorless and transparent after being decolourized and decarbonized in air and hydrogen successively at high temperature. The quality, optical transmissivity and homogeneity of the sapphire boule have remarkably improved.
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Fabrication of PZN-PZT Piezoceramics and Ceramic Fibers
LI Kun,CAO Da-Hu,LI Jin-Hua,CHAN Helen-Lai-Wah
2005 Vol. 20 (5): 10991105
Abstract(
2218 )
PDF(718KB)(
1244
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By using lead acetate, zinc propionate, niobium ethoxide, zirconium propoxide and titanium butoxide as precursors, zinc and niobium modified lead zirconate titanate (PZN-PZT) gel fibers were fabricated by the sol-gel method. Prolyzed and sintered, The PZN-PZT ceramic fibers with a diameter of about 25μm were obtained. The SEM micrographs show that these ceramic fibers are dense and uniform. The X-ray diffraction patterns show that sintering temperatures will affect the crystal structure of PZN-PZT ceramics. When the sintering temperature higher than 1250℃, the sintered ceramics and ceramic fibers have a pure perovskite structure. The densities of the bulk ceramic and ceramic fiber are 7.70×103kg/m3 and 7.80×103kg/m3, which were measured by Archimedes method. The electromechanical coupling coefficient kt, piezoelectric coefficient d33 and relative permittivity ε of the PZN-PZT fiber/epoxy 1-3 composite disk with 63% fibers loaded are 0.65, 403 pC/N and 1300, respectively. The kt, d33 and ε of the PZN-PZT ceramics made from the sol-gel powder are 0.48, 600 pC/N and 2627, respectively.
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Preparation of BaTiO3-Acetylene Black Composite with a Super High Dielectric Constant
HUANG Ji-Quan,DU Pi-Yi,WENG Wen-Jian,HAN Gao-Rong
2005 Vol. 20 (5): 11061112
Abstract(
2509 )
PDF(641KB)(
1264
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The ceramic composite which has a super high dielectric constant was prepared by compounding and sintering Acetylene Black(AB) and BaTiO3 together in the protective atmosphere. Microstructure and morphology of the composite were measured by XRD and SEM, and the dielectric properties were measured by LCZ meter. The results indicate that the prepared samples, are much difficult to form BaTiO3/AB composites when sintering in air atmosphere and at high temperature, because AB is oxidated and volatilized under that case. But the calcination process is improved due to the formation of liquid phases with decomposition and volatilization of AB in the AB doped BT system, AB can however be distributed in the sintered BaTiO3 matrix perfectly when sintering in the protective atmosphere of N2. The BaTiO3/AB ceramic composite with dense structure is hence formed completely while calcining at the temperature range 1200℃ to 1250℃. The dielectric constant of the BaTiO3/AB composite is increased evidently around the percolation threshold. The super high dielectric constant of 35000 can be obtained in BaTiO3/AB composites when AB content between 0.8wt% and 2.0wt%, which is 12 times more than that of BaTiO3 without AB doping.
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Polar Growth Phenomenon in ZnO Varistor
HE Zhong-Wei,XU Ye-Wen,XU Zheng,SUN Dan-Feng
2005 Vol. 20 (5): 11131119
Abstract(
2160 )
PDF(1159KB)(
1183
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The protuberance phenomenon in shape of conic or cylinder was discovered for the first time. It was found by EDS that the protuberance is entity formed by ZnO, not the air bubble. And it was proved that the polar growth of ZnO leads to the protuberance phenomenon. The detailed reasons were probed from internal and external courses. The internal course is the polar structure and morphology of ZnO crystal. The external course is the physical and chemical environment made by Bi2O3 liquid phase, and this conclusion was proved by the comparisons of the samples which fabricated by 97mol%ZnO+3mol%Bi2O3 (in mole) compound and 100mol% (in mole) ZnO compound.
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Structural and Electrochemical Characterization of LiMn2-2xLixNixO4 (0≤x≤0.1) Cathode Materials
TU Jian,CAO Gao-Shao,ZHUANG Da-Gao,ZHAO Xin-Bing
2005 Vol. 20 (5): 11201126
Abstract(
1955 )
PDF(575KB)(
1209
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Lithium and nickel co-doped LiMn2-2xLixNixO4 cathode materials (x= 0, 0.03, 0.05, 0.075, 0.1) were synthesized by a high temperature solid-state reaction route. The microstructures and morphologies of the samples were characterized by X-ray powder diffraction, X-ray absorption fine structure analysis and field emitted scanning electronic microscopy. The bond lengths of the MnO6 octahedrons and the electrochemical performances in both room temperature and elevated temperature (55℃) were characterized and discussed in comparison with LiMn2O4 spinel. The result reveals that LiMn2-2xLixNixO4 samples have a good reversibility. It is suggested that the co-doping of lithium and nickel in LiMn2O4-based compounds could stabilize the spinel structure and improve the capacity retention of the cathode materils.
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Synthesis and Performance of LiCrxMn2-xO4 Cathode Materials for Li-ion Battery
YAO Yao-Chun,DAI Yong-Nian,YANG Bin,CUI Meng-Jia,LI Wei-Hong
2005 Vol. 20 (5): 11271131
Abstract(
2086 )
PDF(646KB)(
1170
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Spinel LiCrxMn2-xO4 cathode materials for Li-ion batteries were synthesized by Pe-chini process, and their crystalline structure, apparent morphology and electrochemical performance were characterized with XRD, SEM and charge-discharge test. Results show that the samples of LiCrxMn2-xO4 possess pure spinel phase, better morphology and uniform distribution of gain sizes, with the increase of Cr content, the lattice parameters are reduced, but Cr content has a little effect on the phase structure and morphology of LiCrxMn2-xO4 . When Cr content increases, the specific capacity of the products will decrease, the stability of spinel structure and cycle performance will be improved.
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Synthesis and Characterization of La0.6M0.4Fe0.8Cr0.2O3-δ(M= Ca, Sr,Ba) by GNP Method and Conductivity
CHEN Yong-Hong,WEI Yi-Jun,GAO Jan-Feng,LIU Xing-Qin,MENG Guang-Yao
2005 Vol. 20 (5): 11321138
Abstract(
2237 )
PDF(382KB)(
1038
)
La0.6M0.4Fe0.8Cr0.2O3-δ(M=Ca, Sr, Ba) fine powders were synthesized by a glycine-nitrate process(GNP). BET test shows that the specific area of the obtained powders is over 20 m2·g-1. XRD test shows that the crystalline structure formed is at the stage of ignition by the method, the powder of La0.6Ca0.4Fe0.8Cr0.2O3-δ(LCFC) is pure cubic perovskite-type after calcined at 850℃ for 2h, and its relative density (sintered at 1100℃) is 95%. The primary powders of LSFC and LBFC are with two-phase structure and with poor sintering activities than that of LCFC at low temperature. The relative density of these ceramics sintered over 1300℃ is 95%. Four-probe technique tests indicate that the conductivity of doped-samples is two orders of magnitude higher than that of LaFeO3, The changes of conductivity with temperature below 700℃ are in accord with the conduction mechanism of small polarons. The electrical conductivity of LCFC at 800℃ is over 50 S/cm which indicates that LCFC may have potential application for IT-SOFC cathode.
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Effects of Addition of Carbon Nanotubes on Properties of MmMn0.4Co0.7Al0.3Ni3.4 Hydrogen Storage Electrode
HUANG Hui,ZHANG Wen-Kui,GAN Yong-Ping,TU Jiang-Ping,ZHANG Xiao-Bin
2005 Vol. 20 (5): 11391144
Abstract(
2205 )
PDF(421KB)(
920
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The electrochemical properties of MmMn0.4Co0.7Al0.3Ni3.4 hydrogen storage electrode with CNTs and Ni additives were invesitigated. The results show that the addition of CNTs in the alloys improves the discharge capacity and initially activation performance. The alloy electrodes with CNTs, CNTs+Ni additives can be completely activated after 11 charge-discharge cycles with maximum capacity of 255.1 and 270.5 mAh/g, respectively. However, activation process of the electrode containing Ni powder needs 24 cycles and the maximum capacity is 245.0 mAh/g accordingly. And also, the addition of CNTs, CNTs+Ni in the alloys modifies the high-rate dischargeability(HRD) performance and reveals the higher discharge voltage. The HRD of electrodes with CNTs, CNTs+Ni, Ni and without any additives are 80.5%, 83.9%, 66.9% and 62.4% at the discharge current of 1000 mAh/g, respectively. From their kinetics analysis of linear polarization curve and electrochemical impedance spectroscopy, the addition of CNTs in the alloys decreases the ohmic resistance and improves the rate of charge transfer reaction on the surface, and contributes to the discharge under the high current conditions.
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Effect of Sintering Process on Dielectric Properties of B2O3-doped Ba1-xSrxTiO3 Graded Ceramics
CHENG Hua-Rong,ZHU Jing-Chuan,JEON Jae-Ho,LAI Zhong-Hong
2005 Vol. 20 (5): 11451152
Abstract(
2040 )
PDF(1010KB)(
1200
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Effect of sintering temperature and heating rate on densification, grain size and dielectric properties of B_2O_3-doped Ba1-xSrxTiO3(x=0~0.4, in step of 0.02) graded ceramics was investigated. With the increase of sintering temperature, B2O3 volatilization and densification improvement resulted in Curie peak elevated and sharpened. With the increasing of dopant content, grains grew up uniformly, and dielectric constant and loss increased. While dopant volatilization, densification process and grain growth were fulfilled synchronously with appropriate heating rate, which conduces to the dielectric improvement and dielectric loss reduction for the graded ceramics. In addition, B2O3 doping lowered at least 150℃ of the sintering temperature, and the dielectric loss was reduced obviously; Curie peak was broadened and flattened remarkably and the temperature coefficient of permittivity was decreased greatly, which means the accuracy and stability of components with such material can be improved.
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Effects of Synthesis Conditions on the Formation and Quality of Zeolite During the Hydrothermal Zeolitization Processes of Fly Ash
WU De-Yi,KONG Hai-Nan,ZHAO Tong-Gang,WANG Chong,YE Chun
2005 Vol. 20 (5): 11531158
Abstract(
2086 )
PDF(578KB)(
1215
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The formation and cation exchange capacity (CEC) of zeolite synthesized after alkaline activation of a Chinese fly ash, as a function of temperature, liquid/solid ratio, NaOH concentration and reaction time in closed systems were investigated. Temperature affected mainly the crystallinity of zeolite formed, liquid/solid ratio affected mainly the type of zeolite, and while NaOH concentration and reaction time influenced both of them. The CEC value of synthesized products increased greatly as a function of temperature, liquid/solid ratio and reaction time until the temperature of 110℃, the ratio of 2.5, and the time of 16h were reached, and then approached to a constant value. The CEC value of synthesized zeolite increased initially with the increase in NaOH concentration, reached its maximum value at a concentration of 2mol·L-1, and then decreased sharply above the concentration. The results show that from the economic point of view, the optimal conditions are as follows: a temperature of 110~120℃, a reaction time of 8~16h, a liquid/solid ratio of 2.5, and a NaOH concentration of 2mol·L-1.
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pH Value Evolution of a Novel Sr-containing Calcium Phosphate Cement Pastes and Cytotoxicities of Their Hardened Bodies
GUO Da-Gang,XU Ke-Wei,YUE Jin,ZHAO Xiao-Yun,HAN Yong
2005 Vol. 20 (5): 11591166
Abstract(
2324 )
PDF(667KB)(
2189
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The online pH value evolutions of a novel Sr-containing calcium phosphate cement (Sr-CPC) pastes together with the extracts of their hardened bodies immersed in the culture medium were measured and the cytotoxicities of various hardened bodies were evaluated by MTT assay. Results obtained from the XRD and FTIR analyses show that most of the Sr-CPC has transformed into Sr-containing apatite solid solution after subjected an immersion process in SBF for 24h. CO32- ion can be detected in the final set product, which is similar to the bone-like apatite. The pH values of various cement pastes basically vary in the range of 6.5~7.8. All extracts exhibit no or low cytotoxicity with a score of 0 or 1 grade according to the six-grade criterion in GB/T 16175-1996. A slight relevance exists among the cytotoxicity and concentration of extracts and acting time.
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Preparation and Property of Sr-Containing Calcium Phophate Cement
ZHAO Xiao-Yun,GUO Da-Gang,HAN Yong,XU Ke-Wei
2005 Vol. 20 (5): 11671173
Abstract(
2298 )
PDF(856KB)(
1169
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A noval Sr-containing calcium phosphate cement (Sr-CPC) was synthesized by mixing tetracalcium phosphate, dicalcium phosphate anhydrous, strontium hydrogen phosphate and phosphate acid. The effects of weight ratio of cement powder to liquid (P/L), the content of Sr and immersion time of samples in simulated body fluid (SBF) on their compressive strength and microstructure of samples were investigated. The results show that there exists an optimum P/L ratio for each cement paste with an excellent workability and setting times, and the setting times of the cement paste obtained at its optimum P/L ratio meet the clinical demands. After immersion in SBF for 24h, the Sr-CPC has transformed into Sr-containing deficient-calcium apatites. The content of Sr and immersion time of samples in SBF have distinct effects on the compressive strength (CS) of the cement hardened bodies. A proper content of Sr and a shorter immersion time are beneficial to improving the CS, and the variation of macrostructure plays a significant role in the CS of the hardened bodies during immersion in SBF.
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Hydraulic Characteristic and Osteoinduction Capacity of Calcium Phosphate/BMP Bioactive Bone Cement
YANG Wei-Zhong,ZHOU Da-Li,YIN Guang-Fu,YIN Shao-Ya,ZHENG Chang-Qiong
2005 Vol. 20 (5): 11741180
Abstract(
1960 )
PDF(947KB)(
1195
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Calcium phosphate(CPC)/BMP bioactive composite bone cement was prepared with ultrafine α-tricalcium phosphate (α-TCP) powders and assist agent premixed with freezed bone morphogenetic protein (BMP) powders. By means of the hydraulic characterization, the composition, cement liquid and promoting solidification agent of the bone cement were optimized. Osteogenesis of the BMP combined bone cement was investigated in the rat muscle pouch. Results show that the novel bone cement with excellent hydraulic properties can be developed with 0.95α-TCP, 0.025CaHPO4, 0.025CaO as the basic composition and 0.25mol/L NaH2PO4/Na2HPO4 solution([P]T=0.5mol/L)as the cement solution, which can satisfy with the harden strength required for clinic surgery. Initial setting time and final setting time of the bone cement are 6min and 30min respectively. The particle size of α-TCP has great influence on the characteristics of bone cement, and the suitable particle size (d50) will be 1.3μm. The compressive strength of the bone cements reaches 33 MPa after soaking in Hank’s solution for 5 days. The morphology of the bone cement becomes a network of hydroxyapatite (HA) after soaking. Ectopic osteogenesis of CPC/BMP composite bone cement is distinct, and lamellar bone can form within 4 weeks, proving the strong osteo-induction capacity of the materials. This bioactive bone cement with good hydraulic characteristics and strong osteogenesis is expected to be a promising bone grafting materials for tissue engineering.
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Preparation and Microstructure of HA-316L Stainless Steel Fibre Asymmetrical Functionally Graded Biomaterial
ZOU Jian-Peng,RUAN Jian-Ming,HUANG Bai-Yun,ZHOU Zhong-Cheng,LIU Yu-Long
2005 Vol. 20 (5): 11811188
Abstract(
2083 )
PDF(1376KB)(
1187
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HA(ZrO2)-316L stainless steel fibre asymmetrical functionally gradient biomaterial(FGM) was successfully fabricated under 1100℃ by low pressure hot isostatic pressing(HIP) technique. Metallographical microscope, SEM, EDXA analysis were carried out to examine the microstructure and elemental contents of the asymmetrical FGM. The results show that asymmetrical stepwise change of volume ratio of 316L stainless steel fibre according to 20%→15%→10%→5% can be corresponded in the FGM. 316L stainless steel fibre is randomly and evenly distributed in the FGM. 316L stainless steel fibre is enwrapped in the HA(ZrO2) matrix and both integrate each other tightly. The interface of 316L stainless steel fibre and HA(ZrO2) matrix is partly concavo-convex. The approach also indicates that some Fe element diffusion of the toughing phase takes place in the HA(ZrO2) matrix and no Ca, P element diffusion of the matrix takes place in 316L stainless steel fibre toughing phase. Both matrix and toughing phase are relatively independent and no chemical reaction is observed in the FGM. With the increase of HA contents, both fracture toughness and Young’s modulus of HA(ZrO2)-316L stainless steel fibre composites are gradually reduced, which leads to mechanical properties relaxation design of the FGM. It is suggested that fibre pulling out and interbedded crack deflexion are the major toughing mechanism in the asymmetrical FGM.
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Nanosized Particles Coating of Inorganic Mineral Filler Surface & Characterization
GAI Guo-Sheng,YANG Yu-Fen,HAO Xiang-Yang,FAN Shi-Min,CAI Zhen-Fang
2005 Vol. 20 (5): 11891194
Abstract(
1944 )
PDF(754KB)(
1185
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Composite mineral particles with nano-structured surface, which effectively improve surface morphology of the originals and increase specific surface area, were successfully prepared by using a chemical method. By wet grinding in a stirring mill, the coalescence between coating particles and the base was discussed. The preliminary conclusion gained shows that the coating particles are not easy to be peeled off from the base because of chemical absorption. The mechanical properties of the composite are greatly improved, when the coated mineral particles filled in polypropylene.
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Morphology and Formation Mechanism of TaC Made by Liquid Phase Infiltration Method in C/C Composites
YAN Zhi-Qiao,XIONG Xiang,XIAO Peng,LI Jiang-Hong
2005 Vol. 20 (5): 11951120
Abstract(
2126 )
PDF(802KB)(
1282
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C/C composites were infiltrated with tantalum-contained organic solution, solidified and thermally treated to produce C/C-TaC composites. The results show that tantalum-contained organic solution easily infiltrates C/C composites and solidifies under 2MPa pressure. After treated at 1500℃, tantalum-contained organic solution tantalum completely turns into TaC with fine sizes and high crystallization, distributing on the layers of pyrolytic carbon with grains or clusters. The morphology of TaC made at 1800℃ and 2000℃ is analogous with that of made at 1500℃ and the grain size of TaC doesn’t grow up obviously. The mechanism research of tantalum-contained organic solution turning into TaC shows that it first turns into tantalum oxide fluoride, a kind of interphase, then Ta2O5 ultimately reduced and compounded by carbon into TaC.
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Preparation of C/C Composites by CVI with Multi-factor Coupling Physical Fields and Deposition Mechanism
XIE Zhi-Yong,HUANG Qi-Zhong,SHU Zhe-An,ZHANG Fu-Qin,HUANG Bo-Yun
2005 Vol. 20 (5): 12011207
Abstract(
2004 )
PDF(925KB)(
1181
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in the felt forming the grads of temperature and electromagnetism, C/C composites were fabricated by chemical vapor infiltration (CVI) with multi-factor coupling physical fields. The textures of pyrolytic carbon were observed by a polarization microscope(PLM), and the graphitization degree and minicrystal size of the C/C composites were analized by XRD. All samples were fabricated at one cycle. The densities of the matrix were measured by on-line coupling with resistance.At last,the mechanism of multi-factor coupling physical fields and deposition of carbon was discussed. The results show that, with multi-factor coupling physical fields, the rate of deposition of pyrolytic carbon can be improved greatly, and when deposited for 20h, C/C composites with densities of more than 1.7g/cm3 will be obtained. Through optimizing the infiltration conditions, some microstructures of pyrolytic carbon can be obtained ,range from rough laminar,smooth laminar, and banded structure. The graphitization degree of the rough laminar can be over 77% after heat treatment at 2300℃ for 2h.
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Preparation and Characterization of C/Si3N4 Composites by Chemical Vapor Infiltration
LIU Yong-Sheng,CHENG Lai-Fei,ZHANG Li-Tong,XU Yong-Dong,LIU Yi
2005 Vol. 20 (5): 12081214
Abstract(
1888 )
PDF(1054KB)(
1090
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C/Si3N4 composites were prepared by chemical vapor infiltration methods (CVI) from SiCl4-NH3-H2 system. The element and phases of the as-processed sample were characterized by EDS and XRD. The phase of the as-processed sample is an amorphous silicon nitride. The phase of the sample heat treated at 1350℃ is also an amorphous silicon nitride. The XRD indicates that the formation of α-Si3N4 and β-Si3N4 occurs after heat treatment at 1450℃. The influences of temperature, time and gas flux on densification, weight and microstructure were investigated. The results show that the gases infiltrate and react in preforms equably, the carbon preforms can be infiltrated uniformly and the uniform C/Si3N4 composites were prepared when the process parameters are as follows: temperatrure 900℃, SiCl4 flow 30mL/min, H2 flow 100mL/min, NH3 flow 80mL/min, time 120h and total pressure 1000Pa.
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Reaction Mechanism of Preparing Porous Silicon Nitride/Silicon Carbide Composite Ceramics
ZHANG Wen,WANG Hong-Jie,JIN Zhi-Hao,BAI Yu
2005 Vol. 20 (5): 12151221
Abstract(
2377 )
PDF(1056KB)(
1659
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The reaction mechanism of preparing porous silicon nitride/silicon carbide (Si3N4/SiC) composite ceramics was investigated by using solidified phenolic resin as carbon source. Argon was used as protective atmosphere. The polymer can pyrolyze to provide free carbon, and farther react with Si3N4 powder coated at different temperatures ranged from 1300℃ to 1780℃. XRD, TEM, the microstructure of the samples, the thermodynamics and kinetics analysis show that the reaction mechanism mainly associates with liquid-solid reaction between C and Si(l) decomposed from Si3N4, and liquid-gas reaction between Si(l) and CO(g) which is the intermediate product during the reactions. Other reaction types involved are solid-solid reaction between C and Si3N4, gas-solid reaction between C and SiO2 coated on the Si3N4 powder, and gas-solid reaction between C and SiO(g) or Si(g). The reactions between pyrolyzed carbon and Si3N4 begin at 1400℃, and form SiC layer. Keeping in higher temperatures can improve the formation of SiC layer and the prolongation of soaking time can increase the thickness of SiC layer significantly.
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Properties of Highly Oriented Transparent KTN/SiO_2 (100) Film Prepared by PLD
WANG Xiao-Dong,PENG Xiao-Feng,ZHANG Duan-Ming
2005 Vol. 20 (5): 12221228
Abstract(
1892 )
PDF(409KB)(
1104
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Highly oriented KTN thin films were produced on the transparent single crystal quartz (100) by the pulsed laser deposition (PLD). XRD analysis indicates that perovskite structure with (h00) orientation is the major phase (>98%) in KTN. The optical and electric measurements show that the remanent polarization and the coercive field are 9.25μC/cm2 and 7.32kV/cm, refractive index 1.776 at incident wave length 1.2μm, thickness 968nm, and growth rate 0.027 nm per pulse. The Current-Voltage characteristics found are Ohmic at lower fields and space-charge-limited at higher fields. This phenomenon was reasonably explained by SCLC theory. The leakage current is lower than 250μA/mm2 at 0--5V, which shows the film has good electric performances. The results of the frequency dependence of dielectric constant demonstrate that the dispersion of electric capacity is large at low frequency but small at high frequency. The dielectric constant is 12600 and the loss tangent is 0.04 at the frequency of 10 kHz.
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Effect of Reactive Temperature on the Characterization of LiCoO2 Film
TAO Ying,CHEN Zhen-Hua,ZHU Bao-Jun
2005 Vol. 20 (5): 12291233
Abstract(
1892 )
PDF(686KB)(
1121
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LiCoO2 films were fabricated on nickel substrates by a hydrothermal-electrochemical method. The film prepared at 80℃ is mainly (003) plane oriented and prepared at 100℃, (101) and (104) plane oriented and prepared at 150℃ (003) plane oriented as well. The (101) plane orientation is favorable for Li+ diffusion through the cathode, and therefore the (101) plane oriented film contributes to the enhanced electrochemical performance. The film with (101) oriented prepared at 100℃ has the capacity of 143mAh/g and no obvious capacity attenuation detected.
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Structure and Property Characterization of Bi2-xSbxTe3 Thermoelectric Films Prepared by Electrodeposition
WANG Wei,HUANG Qing-Hua,JIA Fa-Long,ZHANG Zhi-Rong
2005 Vol. 20 (5): 12341238
Abstract(
1944 )
PDF(470KB)(
1059
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Bi2-xSbxTe3 thermoelectric films were prepared by potentiostatic electrodeposition. The morphology, structure and composition of the electrodeposited films were investigated by ESEM, XPS, XRD, and EDS. And the Seebeck coefficients of Bi2-xSbxTe3 thermoelectric films electrodeposited at different potentials were measured. The results indicate that bismuth, antimony and tellurium can be coelectrodeposited to form Sb doped Bi2Te3 compouds Bi2-xSbxTe3 in the solution containing Bi3+, HTeO+2and SbO+. The doping concentration of Bi2-xSbxTe3 thermoelectric films can be controlled through adjusting electrodeposition potential to affect their thermoelectric properties. The composition of the film electrodeposited at --0.5V is Bi0.5Sb1.5Te3, and it has the largest Seebeck coefficient of 213μV·K-1. With the decrease of electrodeposition potential, the crystalline state of Bi_{2-x}Sb_xTe_3 film will transform from equiaxed crystal into dendritic crystal. The study shows that the electrodeposition process can be successfully used to synthesize the thermoelectric films with better properties.
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Polycrystalline PbI2 Thin Films Deposited by Vacuum Evaporation
LI Yu-Hong,ZHANG Hong,LI Zhen-Sheng,LI Dan-Min,HE De-Yan
2005 Vol. 20 (5): 12391242
Abstract(
1796 )
PDF(234KB)(
1076
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Lead iodide (PbI2) polycrystalline thin films were deposited on glass substrates by vacuum evaporation technique. The structure, surface morphology and composition of the films were characterized by using X-ray diffraction, scanning electron microscope, X-ray photoelectron spectrometer. The results indicate that the films are polycrystalline with a preferred orientation along (001). The measurement of conductivity as a function of temperature shows that the dark conductivity of the film at room temperature is as low as 3.09×10-11(Ω·cm)-1, and the activation energy is 0.78eV.
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Preparation of TiO2 Film on Stainless Steel Webnet and the Degradation of Formaldehyde
ZHANG Jian-Ping,SUN Zhao-Mei,SHI Li-Yi,JIA Gui-Ling,XIE Xiao-Feng,RAO Wei-Wei,ZHU Yong-Fa
2005 Vol. 20 (5): 12431249
Abstract(
2091 )
PDF(790KB)(
1051
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Photocatalytic titanium dioxide films coated on stainless steel webnet were prepared by a sol-gel route. SEM, XRD and TG-DTA were employed to characterize the samples. The effects of the films prepared with different proceedings on photoactivity were investigated by formaldehyde photodegradation, such as the molecular weight of PEG, the amount of PEG, moisture content, the thickness of the films and the annealing temperatures. The formaldehyde photodegradation ratio can reach above 90% by the TiO2-based films. XRD patterns and SEM observation indicate that the TiO2 films with mesoporous structure are composed of mixed rutile and anatase crystals.
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Preparation and Structural Characterization of Al2O3-SiO2 Composite Membrane
YU Jian-Chang,XU Wei-Jun,HU Sheng-Wei,HUANG Qing-Ming
2005 Vol. 20 (5): 12501256
Abstract(
1882 )
PDF(449KB)(
1106
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Al2O3-SiO2 composite membrane was prepared by sol-gel process using aluminium isopropoxide and tetraethoxysilane as raw materials. The phase constitution, thermal stability, and the pore structure were characterized by means of XRD, DTA-TGA, IR, BET etc. The results show that the phase constitution of the composite membrane was SiO2 and γ-Al2O3 after calcined at 550℃ for 10h, and the particle size range from 2nm to 4nm. The XRD results of the composite membrane (Al2O3/SiO2=3:2) calcined at different temperatures show that the membrane is constituted of γ-AlOOH and γ-Al2O3 at 400℃, γ-Al2O3 at 550℃ to 1150℃, γ-Al2O3 and α-Al2O3 at 1220℃, mullite and α-Al2O3 at 1300℃. Al2O3-SiO_2 composite membrane is constituted of Al--O and Si--O networks, and no Al--O--Si network found membrane. The composite membrane has high thermal stability, and the pore structure of the membrane can influence on its constitution and the thermal treatment temperatures.
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Influence of Ag Substrate Textures and Surface Condition on Properties of YBCO Film
LIU Min,DONG Jie,ZHAO Yue,LIU Dan-Min,ZHOU Mei-Ling
2005 Vol. 20 (5): 12571262
Abstract(
2014 )
PDF(733KB)(
1093
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In order to study the influence of the texture and surface morphology of Ag substrates on the YBCO film properties, YBCO films were deposited on three different Ag substrates. The YBCO film deposited on Ag substrate annealed in vacuum has a poor texture and low Jc. in addition, the film is loose and unconnected. The YBCO films deposited on Ag substrate annealed in Ar atmosphere have strong c biaxial texture and higher Jc 1.2×104A/cm2. The texture of YBCO film deposited on the cold rolled Ag substrate is not as strong as the texture of the film deposited on Ag substrate annealed in Ar atmosphere. Due to its smooth surface, the YBCO film deposited on the cold rolled Ag substrate still has higher Jc of 1.5×104A/cm2.
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Effects of Atomic Hydrogen on Growth of Nanodiamond Films
LIN Liang-Wu,TANG Yuan-Hong,ZHU Li-Bing
2005 Vol. 20 (5): 12631269
Abstract(
2249 )
PDF(535KB)(
1225
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The effects of atomic hydrogen on the growth of nanodiamond films were explored under different conditions of preparation. It is believed hydrogen-poor is not the necessary factor for preparation of nanodiamond films. The mechanisms of atomic hydrogen and Ar are different between the condition of hydrogen-poor and hydrogen-rich. Substrate bias fixed, can promote the production of H+. H+ can etch sp2 carbon stronger than sp3 carbon, and can result in surfacspe defects. Therefore, the condition of hydrogen-rich will be assistant to the nucleation and growth of nanodiamond films.
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Effects of Boron Doping on the Growth Characteristic of Diamond Film
LIU Wei-Ping,YU Qing-Xuan,TIAN Yu-Quan,LIAO Yuan,WANG Guan-Zhong,FANG Rong-Chuan
2005 Vol. 20 (5): 12701274
Abstract(
2104 )
PDF(522KB)(
1215
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Boron-doped diamond thin films, synthesized by the HFCVD method, were analyzed by SEM and XRD. The results show that, when the boron concentration in the films increases, the crystallite orientation changes from (100) to (111), then tends to disorder. The doping of boron reduces the growth parameter α. The stress in the films is relaxed by twin crystals in the boron doping films. Consequently the shift of center phonon line of Raman spectrum becomes smaller.
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Osseointegration of Plasma-sprayed Titanium Coating after Alkali Modification
XUE Wei-Chang,ZHENG Xue-Bin,LIU Xuan-Yong,DING Chuan-Xian
2005 Vol. 20 (5): 12751280
Abstract(
1858 )
PDF(984KB)(
1095
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Plasma sprayed titanium coatings were modified by alkali treatment process. The bone bonding ability of titanium coatings was investigated in vivo implantation in dog’s femur. The bond strength between bone and titanium coatings was also measured by push-out test. The results obtained indicate that the alkali-modified coating not only bond directly to bone, but also accelerate the ingrowth of bone. After 1 month of implantation, the alkali-modified coatings show good osseointegration and higher shear strength. The mechanism of improving osseointegration of alkali-modified titanium coating described can be attributed to the changes in surface micro-topography and chemistry composition after alkali modification.
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